IP Library Granted Patent US 9,074,265
Granted Patent B2
US 9,074,265 · App. 14/045,297 · Granted Jul 7, 2015

Processes for preparing highly pure lithium carbonate and other highly pure lithium containing compounds

Inventors: Stephen Harrison (Benicia, CA); Robert Blanchet (Palm Desert, CA)
Assignee: Simbol, Inc.
C22B26/12C01B35/063C01D15/02C01D15/04C01D15/08C01G45/1228C01G51/42C01P2006/80C25B1/02C25B1/26
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Quick Facts
Patent No.
US 9,074,265
App. No.
14/045,297
Granted
Jul 7, 2015
Kind
B2
Abstract

The invention generally relates to methods of selectively removing lithium from various liquids, methods of producing high purity lithium carbonate, methods of producing high purity lithium hydroxide, and methods of regenerating resin.

Claims (33)

1. A method of producing high purity lithium carbonate, the method comprising the steps of:

supplying a first aqueous solution containing lithium sulfate to an electrochemical cell;

electrolyzing the first aqueous solution to produce a second aqueous solution containing sulfuric acid and a third aqueous solution containing high purity lithium hydroxide;

reacting the third aqueous solution containing high purity lithium hydroxide with carbon dioxide to produce a fourth aqueous solution containing lithium bicarbonate;

separating the fourth aqueous solution from the carbon dioxide and lithium carbonate solids using a gas-liquid-solid separator;

filtering the fourth aqueous solution to remove trace impurities; and

feeding the filtered fourth aqueous solution to a precipitation reactor to precipitate highly pure lithium carbonate.

2. The method of claim 1 , wherein the step of reacting the third aqueous solution containing high purity lithium hydroxide with carbon dioxide produces the fourth aqueous solution having a pH of 8.5.

3. The method of claim 1 , wherein the step of reacting the third aqueous solution containing high purity lithium hydroxide with carbon dioxide is carried out at a temperature of about 15° C. to about 30° C.

4. The method of claim 1 , wherein the step of reacting the third aqueous solution containing high purity lithium hydroxide with carbon dioxide is carried out at a temperature of at least about 20° C.

5. The method of claim 1 , wherein the third aqueous solution containing high purity lithium hydroxide comprises at least 2 wt % lithium hydroxide.

6. The method of claim 1 , wherein the third aqueous solution containing high purity lithium hydroxide comprises at least 4 wt % lithium hydroxide.

7. The method of claim 1 , wherein the filtered fourth aqueous solution is passed through an ion exchange column to remove divalent ions before feeding the filtered fourth aqueous solution to a precipitation reactor.

8. The method of claim 7 , wherein the divalent ions removed from the filtered fourth aqueous solution includes one or more of iron, silica, magnesium, manganese, calcium and strontium.

9. The method of claim 1 , wherein the highly pure lithium carbonate produced in the precipitation reactor contains lithium in excess of 99.9% purity.

10. The method of claim 1 , wherein the highly pure lithium carbonate produced in the precipitation reactor contains lithium in excess of 99.99% purity.

11. The method of claim 1 , wherein the highly pure lithium carbonate produced in the precipitation reactor contains lithium in excess of 99.999% purity.

12. The method of claim 1 , wherein the precipitation reactor is maintained at a temperature of at least about 95° C. to precipitate highly pure lithium carbonate.

13. The method of claim 1 , wherein the electrochemical cell includes a cathode, an anode, and a semi-permeable ion selective membrane.

14. The method of claim 1 , wherein the anode contains titanium.

15. The method of claim 1 , wherein the cathode contains nickel.

16. The method of claim 1 , wherein the highly pure lithium carbonate produced in the precipitation reactor contains lithium carbonate particles having an average diameter of less than about 100 μm.

17. The method of claim 1 , wherein the highly pure lithium carbonate produced in the precipitation reactor contains lithium carbonate particles having an average diameter of less than about 50 μm.

18. The method of claim 1 , wherein the highly pure lithium carbonate produced in the precipitation reactor contains lithium carbonate particles having an average diameter of less than about 10 μm.

19. The method of claim 1 , wherein the trace impurities removed from the fourth aqueous solution includes at least one or more of phosphates and borates.

20. A method of producing high purity lithium carbonate, the method comprising the steps of:

supplying a first aqueous solution containing lithium sulfate to an electrochemical cell;

electrolyzing the first aqueous solution to produce a second aqueous solution containing sulfuric acid and a third aqueous solution containing high purity lithium hydroxide;

reacting the third aqueous solution containing high purity lithium hydroxide with carbon dioxide to produce a fourth aqueous solution containing lithium bicarbonate;

separating the fourth aqueous solution from the carbon dioxide and lithium carbonate solids;

filtering the fourth aqueous solution to remove trace impurities;

feeding the filtered fourth aqueous solution to a precipitation reactor to precipitate highly pure lithium carbonate and a fifth aqueous solution containing lithium bicarbonate; and

supplying the fifth aqueous solution to a reverse osmosis apparatus to produce highly pure lithium carbonate, wherein the reverse osmosis apparatus is operable to remove CO 2 from the fifth aqueous solution and cause lithium carbonate to precipitate.

Assignments (7)
LICENSE Recorded Mar 23, 2023
From: TERRALITHIUM LLC
To: ENERGYSOURCE MINERALS LLC
Reel/Frame 063153/0792 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 26, 2020
From: ALL AMERICAN LITHIUM LLC
To: TERRALITHIUM LLC
Reel/Frame 052749/0163 →
CHANGE OF NAME Recorded Apr 9, 2019
From: ALGER ALTERNATIVE ENERGY LLC
To: ALL AMERICAN LITHIUM LLC
Reel/Frame 050124/0185 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 27, 2017
From: SIMBOL, INC.
To: ALGER ALTERNATIVE ENERGY, LLC
Reel/Frame 043117/0923 →
RELEASE OF SECURITY INTEREST Recorded Jul 17, 2017
From: GEOTHERMAL ENERGY PROJECT, LLC
To: SIMBOL, INC.
Reel/Frame 043022/0797 →
SECURITY INTEREST Recorded Apr 18, 2014
From: SIMBOL, INC.
To: GEOTHERMAL ENERGY PROJECT, LLC
Reel/Frame 032705/0714 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 3, 2013
From: HARRISON, STEPHEN; BLANCHET, ROBERT
To: SIMBOL INC
Reel/Frame 031708/0875 →
Continuity (4)
Continuation 13305465 · Nov 28, 2011
Continuation 13029908 · Feb 17, 2011
Provisional Application 61305213 · Feb 17, 2010
Related Publication 20140037521A1 · Feb 6, 2014